title: Optimization of detection conditions and single-laboratory validation of a multiresidue method for the determination of 135 pesticides and 25 organic pollutants in grapes and wine by gas chromatography time-of-flight mass spectrometry.
abstract: This paper describes single-laboratory validation of a multiresidue method for the determination of 135 pesticides, 12 dioxin-like polychlorinated biphenyls, 12 polyaromatic hydrocarbons, and bisphenol A in grapes and wine by GC/time-of-flight MS in a total run time of 48 min. The method is based on extraction with ethyl acetate in a sample-to-solvent ratio of 1:1, followed by selective dispersive SPE cleanup for grapes and wine. The GC/MS conditions were optimized for the chromatographic separation and to achieve highest S/N for all 160 target analytes, including the temperature-sensitive compounds, like captan and captafol, that are prone to degradation during analysis. An average recovery of 80-120% with RSD < 10% could be attained for all analytes except 17, for which the average recoveries were 70-80%. LOQ ranged within 10-50 ng/g, with < 25% expanded uncertainties, for 155 compounds in grapes and 151 in wine. In the incurred grape and wine samples, the residues of buprofezin, chlorpyriphos, metalaxyl, and myclobutanil were detected, with an RSD of < 5% (n = 6); the results were statistically similar to previously reported validated methods.
authors.affiliation: University of Pune, Department of Environmental Sciences, Pune-411 007, India.
authors.forename: Soma
authors.initials: S
authors.lastname: Dasgupta
authors.forename: Kaushik
authors.initials: K
authors.lastname: Banerjee
authors.forename: Kondiba N
authors.initials: KN
authors.lastname: Dhumal
authors.forename: Pandurang G
authors.initials: PG
authors.lastname: Adsule
mesh_terms: D001559:Benzhydryl Compounds; D005506:Food Contamination / Q000032:analysis* / Q000706:statistics & numerical data; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods* / Q000706:statistics & numerical data; D006801:Humans; D007753:Laboratories; D008452:Maximum Allowable Concentration; D010573:Pesticide Residues / Q000032:analysis; D010575:Pesticides / Q000032:analysis*; D010636:Phenols / Q000032:analysis; D011078:Polychlorinated Biphenyls / Q000032:analysis; D011084:Polycyclic Aromatic Hydrocarbons / Q000032:analysis; D013696:Temperature; D027843:Vitis / Q000737:chemistry*; D014920:Wine / Q000032:analysis*; D000098826:Bisphenol A Compounds
chemical_list: D001559:Benzhydryl Compounds; D010573:Pesticide Residues; D010575:Pesticides; D010636:Phenols; D011078:Polychlorinated Biphenyls; D011084:Polycyclic Aromatic Hydrocarbons; C006780:bisphenol A; D000098826:Bisphenol A Compounds